| Ligustri Lucidi Fructus(LLF)is the dry and mature fruit of Ligustrum lucidum Ait,a plant of the oleaceae family.It is sweet and bitter in flavor,cool in nature and attributes to the liver and kidney meridians.Its main effects are to invigorate liver and kidney,strengthen muscles and bones,and improve the eyesight.It can be used to cure fever due to the deficiency of Yin,weakness of the waist and knees,the deficiency of kidney manifested as spermatorrhea,failure of eyesight,etc.Current studies showed that LLF mainly contains compounds such as terpenoids,fatty acids,flavonoids and volatile oils,which have the effects of antioxidant,immune enhancement,growth promotion and improvement of meat and egg quality.In this experiment,the preparation process optimization and quality control of extract of Ligustrum Ligustri Fructus,and the preparation process optimization and quality control of extract granules of Ligustrum Ligustri Fructus were studied,the aim is to provide the basis for the further development and utilization of Ligustrum Ligustri Fructus.(1)The experiment optimize the preparation process of LLF extract: On the basis of single factor test,the transfer rate of ligustrin,the transfer rate of oleanolic acid and the yield of dry extract in LLF extract are used as evaluation indicators.The orthogonal test method optimizes the technological conditions for the preparation of LLF extract.The results showed that the influence of various factors on the extraction of LLF was in the order of ethanol concentration > extraction time > extraction temperature > material-to-liquid ratio.The influence of ethanol concentration and extraction time on the extraction of LLF was significantly different(P < 0.05);The optimal process conditions are: ethanol concentration 70%,extraction time 1h,material-to-liquid ratio 6 times the amount,extraction temperature 80℃;Under the optimal technological conditions,the transfer rates of ligustrin and oleanolic acid in the extract of LLF were 69.74% and 94.31%,respectively.The average yield of dry extract was 45.67%,which was in line with the predicted value.Basically consistent,indicating that the method is suitable for the preparation of LLF extract.(2)Quality control research on LLF extract: Thin-layer chromatography(TLC)and high performance liquid chromatography(HPLC)were used to identify and determine the content of ligustrin and oleanolic acid in LLF extract.The results showed that the extract of LLF and the reference substance of ligustrin and the reference substance of oleanolic acid showed the same color spots on the corresponding chromatographic positions,and the negative without interference;Standard curve for determination of ligustin and oleanolic acid are y=521433x+23028(r=0.9996)and y=198689x-2775(r=0.9999).The content is within the range of 0.35-9.03mg/g and 0.33-7.22mg/g.The linear relationship is good.The experimental results show that the precision,repeatability and sample recovery rate are good respectively,indicating that this method is suitable for the determination of the content of ligustrin and oleanolic acid in the LLF extract.(3)The experiment optimize the preparation process of LLF extract granules:on the basis of pre-experiments,the ratio of extract excipients,ratio of excipients,ethanol concentration and ethanol dosage that affect the quality of granules are investigated,and the molding rate of granules is determined.Bulk density,angle of repose,melting and moisture absorption rate evaluation index to calculate the comprehensive score,the orthogonal test method was used to optimize the preparation process of LLF extract granules,and the preparation process with the highest comprehensive score in the orthogonal test was carried out.The results showed that the influence of various factors on the preparation of LLF granules was in the order of the ratio of extract excipients > the ratio of excipients > the ethanol concentration >the amount of ethanol.The effect of extract and excipient ratio on the preparation of LLF granules is significantly different(P<0.05);The best process conditions are: the ratio of extract: excipients is 1:1.5,the ratio of β-cyclodextrin:D-mannitol is 1:2,the ethanol concentration is 95%,and the amount of ethanol is 24%;the average comprehensive score of the three verification tests is 97.25,which is basically consistent with the predicted value,indicating that this method is suitable for the preparation of LLF extract granules.(4)Quality control research on LLF extract granules: The general inspection of LLF extract granules was carried out,and the TLC method and HPLC method were used to identify and determine the content of ligustin and oleanolic acid in LLF extract granules.The results show that the LLF extract granules are dry in appearance,uniform in size,purple-black in color,and there is no softening,agglomeration,moisture absorption,deliquescence,etc.The water content is 1.74%,and the molding rate is 95.24%,comply with the regulations in the second part of the 2015 edition of the Pharmacopoeia of the People’s Republic of China;LLF extract granules and the reference substance of ligustrin and the reference substance of oleanolic acid all show the same color spots on the corresponding chromatographic positions,and there is no interference in the negative;The method precision,repeatability and sample recovery rate of the determination of the content of ligustrin and oleanolic acid in LLF extract granules are good,indicating that the method is suitable for its determination.This experiment optimized and determined the preparation process of LLF extract and its granules,and established the thin-layer chromatographic identification and content determination methods of LLF extract and granules. |
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